Harold t



Patented Mar. 10, 1925.

UNITED STATES PATENT OFFICE.

HAROLD T. MZAITLAND, OF SHARON HILL, PENNSYLVANIA, ASSIGNOR TO SUN OIL COMPANY, OF PHILADELPHIA, PENNSYLVANIA, A CORPORATION OF NEW JERSEY.

PROCESS OF MANUFACTURING A NEW COMPOSITION FROM MINERAL OIL.

No Drawing.

T 0 all whom it may concern:

Be it known that I, HAROLD T. MAI LAND, a citizen ofthe United States, residing at Sharon Hill, county of Delaware, and State of Pennsylvania, have invented a new and useful Improvement in Processes of Manufacturing a New Composition from Mineral Oil, of which the following is a full, clear, and exact description.

The object of my invention is to produce a mineral oil derivative that is adapted to the manufacture of a linseed oil substitute and a drying oil and probably to many other useful purposes.

The invention comprises a process for making this derivative. It is. preferred to practice the-process in accordance with the description herein, although it will be understood that precise adherence to the specified details of treatment is not required in order to produce the product sought.

In practicing the process I start with certain products that have been extracted by me from crude petroleum and that react with alkalies to form soaps. These prodnets are believed to be organic acids of the resin group present in the crude petroleum. They are known as saponifiable oils, organic acids, fatty acids, etc., and are herein after, for convenience, designated as fatty acids. One method of extracting these fatty acids is set forth in my Patent No. 1,425,882, issued August 15, 1922. I prefer, however, to extract these fatty acids, in the form of soaps, by the process set forth in an application filed by me March 24, 1923, Serial No. 627,317. In accordance with the preferred mode of executing this process therein described, I first distill the crude petroleum to substantial dryness. After con- (lensing the vapors, the condensate is run into an agitator and treated with an alkali, such as caustic soda, calcium h droxid, potassium hydroxid, sodium car onate, etc., preferably caustic soda. After settlement, the precipitate, which is drawn ofi comprises mainly the fatty acid soaps sought to be recovered with a very small proportion of mineral oil.

These "fatty acid soaps are run into a conical agitator, to which is added asuitable solvent, such as one of the light hydrocarbons known as turpentine substitutes, which, in the distillation of crude petro- Application filed March 24., 1923. Serial No. 627,320.

F. by means of a steam coil or with live steam.

To the heated solution is added very slowly a 5 Baum solution of a mineral acid, preferably sulfuric acid, the solution being thoroughly agitated with live steam or air until the excess sodium hydrate present is almost neutralized. This can be determined by using, in the titration, alcohol instead of water, in order to prevent decomposition of the soap. Approximately ten per cent of the above acid solution will be necessary to complete the neutralization. Care should be taken to avoid the use of too much acid, as otherwise the fatty acids will be precipitated through splitting up or decomposition of the soap. The end point is easily observable. At its approach the solution assumes a drab translucent appearance, and a trace of pink should remain on the phenolphthalein paper, which I find is most convenient in this neutralizing step.

A 7 Baum solution of aluminum sulfate, Al (S0,) is then added very slowly while the above mentioned agitation continues. This solution is made by using approximately ten per cent aluminum sulfate in ninety per cent water gravimetrically meas ured. If a precipitate (curdy in appearance) appears before the first quarter of the total aluminum sulfate solution has .been added, it shows that the solution is being introduced too rapidly, and the addition of this" solution should be discontinued until the curds have been redissolved in the mixtu're. The addition of the solution. is then continued slowly until an amount, measured by volume, equal to about twenty per cent of the total amount of soaps, has been added. A break in the mixture will be noticed during theintroduction of the last seventy-five per cent of the total amount of aluminum sulfate and a brown homogeneous viscous liquid, which I designate aluminum resinate, will separate andcome to the top of the mixture. The salt water remaining in the bottom should be sampled and tested with a little of the aluminum sulfate. solution in Order to determine the end point of precipitation. Completion of the precipitation will be denoted by a light yellow color of the now transparent salt water as well as by the appearance of a very light colored precipitate which will begin to appear as soon as the resinate has been thrown out of solution. The appearance of the light colored precipitate denotes the point at which the addition of the sulfate solution should be discontinued, as the above mentioned light colored precipitate is aluminum hydroxide with a little ferrous hydroxide present as an impurity, and its presence in the resinate would probably be detrimental for certain purposes. After completion of precipitation, the compound should be agitated for about an hour to insure a one hundred per cent conversion of the soda soap to aluminum resinate. After permitting settlement, the

salt water is drawn off, and the supernatant solution is washedwwith; hot water or steam until free from sulfates. This is ascertained by testing the wash water with a barium chlorid solution. By salt water is meant the water containing the chemical salt that has dissolved therein.

The washed solution is thenpumped to a still and should be steamed for about an hour and settled for about two hours. The condensed water is then drawn off 'and the solvent distilled off with fire and-steam. If a hard dry material is desired, the still should be sampled until the residuum has reached the proper state. The still at no time should be superheated, as the distillation should be so conducted as to insure a good, dry, flexible compound with a good color.

If a quick drying oil is desired, the still is cooled (always having a certain amount of steam passing through the residuum) to a point where the necessary solvent can be added. This should be done slowly. The light end of the solvent should not be distilled over, as the rapid drying features of the material would be impaired by such treatment.

If gasoline be added to the compound until the solution has about the consistency of linseed oil, a good linseed oil substitute is produced. I have found the solution to have special utility for coating machined work to prevent it from rusting before going into use. When used as a drying oil,

any commercial dryer may be added by the 2. The process of manufacturing a composition adapted for use in making a linseed oil substitute, drying oil, etc., which comprises distilling crude petroleum to drive off a distillate containing fatty acids,

treating the distillate with an alkali in order to saponify the contained fatty acids, separating out the fatty acid soaps, dissolving the soa'ps in a hydrocarbon solvent, treating thev solution successively with a mineral acid and aluminum sulfate, separating out of the water containing the salt} and distilling off the solvent.

3. The process of manufacturing a composition adapted for use in making a linseed oil substitute, drying oil, etc., which comprises manufacturing fatty acid soaps from mineral oil, dissolving the soaps in a hydrocarbon solvent, heating and adding a solution of .a mineral acid with agitation, adding a solution of aluminum sulfate with agitation, separating the water containing the salt from the solution and distilling oil the solvent.

4. The process of manufacturing a composition adapted for use .in' making a lin seed oil substitute, drying oil, etc., which comprises manufacturing fatty acid soaps from mineral oil, dissolving the soaps in a hydrocarbon solvent, heating and adding gradually a solution of a mineral acid with agitation, adding gradually a solution of aluminum sulfate with agitation and continuing the agitation until substantially all the soa is converted to aluminum resinate, separating out the water containing the salt, washing the solution substantially free from sulfates, steaming and then settling the solution, drawing off the condensed water, and distilling oil' the solvent.

In testimony of which invention,I have hereunto set my hand, at Philadelphia, Pa., on this 8th day of March, 1923.

HAROLD T. MAITLAND. 

